HRID495658

反应详情

EQUATION

反应方程式

HRID 495658 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of 3-[2-(diethylamino)ethyl]-2-oxo-7-(trifluoromethyl)-1-[3-(trifluoromethyl)benzyl]-2,3-dihydro-1H-benzimidazole-5-carbonitrile (226.3 mg) in t-butanol (10 ml) was stirred with heating at 60° C. To the solution was added powdered potassium hydroxide crashed in mortar (652.3 mg), and the mixture was stirred with heating at 60° C. for 2 hours. To the reaction mixture were added saturated aqueous sodium bicarbonate solution and water, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by HPLC using condition 2 to give the title compound (145.8 mg, 51%).

WORKUP

后处理

  1. additionTo the solution was added
  2. temperaturewith heating at 60° C. for 2 hours
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resultant residue was purified by HPLC